节点文献
InP纳米材料的合成及性能研究
Synthesis and Properties Study of InP Nanomaterials
【作者】 于彦龙;
【导师】 高发明;
【作者基本信息】 燕山大学 , 应用化学, 2014, 博士
【摘要】 作为重要的III-V族化合物半导体纳米材料之一,InP纳米材料因其在纳米电子器件和纳米光电子器件等方面的应用,已经成为当前纳米科学与技术研究领域的热点之一。本文分别采用化学气相沉积法和溶剂热法合成出了具有不同晶体结构的纳米线、纳米针、纳米管和纳米梳等InP纳米材料,并研究了合成工艺条件对材料的晶体结构、形貌及光学性能等方面的影响。采用单温区加热化学气相沉积法,在In粉用量为1.0mmol,In粉与红磷摩尔比为1:1.3,合成温度650℃工艺条件下合成出了具有多晶结构的InP纳米线;采用双温区加热化学气相沉积法,在In粉用量为1.0mmol,In粉与红磷摩尔比为1:1.3:2.6,加热1区温度650℃,加热2区温度700℃工艺条件下合成出了具有单晶结构的InP纳米线;采用预加热双温区加热化学气相沉积法,先将In粉预加热至200℃保温30min,然后在In粉用量为1.0mmol,In粉与红磷摩尔比为1:1.3:2.6,加热1区温度650℃,加热2区温度700℃工艺条件下合成出了包含层错的孪晶结构InP纳米线。实验结果表明,采用化学气相沉积法通过改变工艺条件,可以合成出不同直径、不同长度和不同晶体结构的InP纳米线。采用溶剂热合成法,以2.0mmol In粉,0.75mmol白磷为原料,以苯为溶剂,以2.0mmol KBH4为还原剂,以2.0mmol十六烷基三甲基溴化铵为表面活性剂,在180℃保温12h,然后升温至380℃保温6h工艺条件下合成出了具有单晶结构的InP纳米线。实验结果表明,使用十六烷基三甲基溴化铵有利于InP纳米材料线状形貌的形成;采用溶剂热法通过改变工艺条件,可以合成出不同直径和不同长度的InP纳米线。采用溶剂热合成法,以2.0mmol In粉,0.75mmol白磷为原料,以苯为溶剂,以2.0mmol KBH4为还原剂,以2.0mmol十六烷基三甲基溴化铵为表面活性剂,在200℃保温12h,然后升温至350℃保温12h工艺条件下合成出了具有单晶结构的InP纳米针;采用溶剂热合成法,以2.0mmol In粉,3.0mmol红磷为原料,以苯为溶剂,以2.0mmol的KBH4为还原剂,以4.0mmol十六烷基三甲基溴化铵为表面活性剂,在200℃保温12h,然后升温至280℃保温12h工艺条件下合成出了单晶结构InP纳米管;采用预加热双温区加热化学气相沉积法,以1.0mmol In粉和3.0mmol红磷为原料,先将In粉预加热至160℃保温30min,然后将加热1区温度升至650℃,加热2区温度升至700℃,保温12h,合成出了包含层错的孪晶结构InP纳米梳。实验结果表明,通过选择不同的合成方法和工艺条件,可以实现对InP一维纳米材料的形貌及晶体结构的控制合成。利用Raman光谱分析法研究了InP纳米线、纳米针、纳米管和纳米梳的Raman光谱。结果表明,相比块体材料而言,InP一维纳米材料的Raman光谱特征峰峰位均发生了不同程度的红移现象。利用PL光谱分析法研究了InP纳米材料的光致发光性能。结果表明,相比块体材料而言,InP一维纳米材料的PL光谱发射峰峰位均发生了不同程度的蓝移现象。利用紫外-可见分光光度计研究了InP纳米线的光催化性能。结果表明,在紫外灯光照射下,InP纳米线对RhB染料的降解具有一定的光催化作用。
【Abstract】 As one of important III-V compound semiconductor nanomaterials, InPnanomaterials have become one of a hot topic in the field of nanoscience andnanotechnology because of its application in electronic and optoelectronic nanodevicesetc.. In this paper, InP nanomaterials with different crystal structure, such as nanowires,nanoneedles, nanotubes and nanocombs and so on, have been synthesized by chemicalvapor deposition method and solvothermal method respectively, while the influence ofsynthetic conditions on the crystal structure, morphology and optical properties ofnanomaterials were studied.InP nanowires with polycrystalline structure have been synthesized by single heatingzone chemical vapor deposition method, in the conditions of1.0mmol In powder and Inpowder, red phosphorus molar ratio of1:1.3, the synthesis temperature of650℃. InPnanowires with single crystal structure have been prepared by double heating zoneschemical vapor deposition method, in the conditions of1.0mmol In powder and Inpowder, red phosphorus molar ratio of1:1.3:2.6, the synthesis temperature of650℃atheating area1and700℃at heating area2. InP nanowires with twin structures stackingfaults phase have been prepared by double heating zones chemical vapor depositionmethod and the In powder preheated to200℃and maintained for30minutes, which isabove the melting point temperature of In, in the conditions of1.0mmol In powder and Inpowder, red phosphorus molar ratio of1:1.3:2.6, the synthesis temperature of650℃atheating area1and700℃at heating area2. Experiments results show that, InP nanowireswith different diameter, length and crystal structures can be synthesized using a chemicalvapor deposition method by changing the synthesis conditions.InP nanowires with single crystalline structure have been prepared by solvothermalsynthesis method, in the conditions of2.0mmol In powder and0.75mmol whitephosphorus as raw materials, benzene as solvent,2.0mmol KBH4as reducing agent,2.0mmol CTAB as surfactant, at180℃for12h, then at380℃for6h.Experiments resultsshow that, CTAB is beneficial to the formation of InP nanomaterial linear morphology; InP nanowires with different diameter and length can be synthesized by a solvothermalmethod by changing the synthesis conditions.InP nanoneedles with single crystal structure have been prepared by solvothermalsynthesis method, in the conditions of2.0mmol In powder and0.75mmol whitephosphorus as raw materials, benzene as solvent,2.0mmol KBH4as reducing agent with,2.0mmol CTAB as surfactant, at200℃for12h, then at350℃for12h;InP nanotubeswith single crystal structure have been prepared by solvothermal synthesis method, in theconditions of2.0mmol In powder and3.0mmol red phosphorus as raw material, benzeneas solvent,4.0mmol CTAB as surfactant, at200℃for12h, then at280℃for12h;InPnanocombs with twin structure containing stacking faults have been prepared by doubleheating zones chemical vapor deposition method and the In powder preheated to160℃and maintained for30minutes, which is about equal to the melting point temperature of In,in the conditions of In powder and red phosphorus molar ratio of1:1.3:2.6, the synthesistemperature of650℃at heating area1and700℃at heating area2for12h. Experimentsresults show that, the morphology and crystal structure of InP one-dimensionalnanomaterials can be controlled by selecting different synthesis methods and conditions.Raman spectra of InP nanowires, nanoneedles, nanotubes and nanocombs werestudied using Raman spectroscopy analysis method. The results show that, compared withthe bulk materials, red shift phenomenon of Raman spectrum characteristic peak positionof InP one-dimensional nanomaterials occurred in different degrees. PL spectra of InPone-dimensional nanomaterials are studied using photoluminescence spectroscopy. Theresults show that, compared with bulk materials, blue shift phenomenon of PL emissionpeak position were observed in different degrees. Photocatalytic performance of InPnanowires were studied by ultraviolet-visible pectrophotometer. The results show that,under ultraviolet light irradiation, InP nanowires have photocatalysis to degradation ofRhB dye.
【Key words】 InP nanomaterials; Chemical vapor deposition method; Solvothermal method; Controllable synthesis; Optical performance;